CN112080002A - Water-soluble corrosion-inhibition and sterilization integrated agent and preparation method thereof - Google Patents
Water-soluble corrosion-inhibition and sterilization integrated agent and preparation method thereof Download PDFInfo
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- CN112080002A CN112080002A CN202010852267.9A CN202010852267A CN112080002A CN 112080002 A CN112080002 A CN 112080002A CN 202010852267 A CN202010852267 A CN 202010852267A CN 112080002 A CN112080002 A CN 112080002A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G73/00—Macromolecular compounds obtained by reactions forming a linkage containing nitrogen with or without oxygen or carbon in the main chain of the macromolecule, not provided for in groups C08G12/00 - C08G71/00
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N47/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom not being member of a ring and having no bond to a carbon or hydrogen atom, e.g. derivatives of carbonic acid
- A01N47/40—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom not being member of a ring and having no bond to a carbon or hydrogen atom, e.g. derivatives of carbonic acid the carbon atom having a double or triple bond to nitrogen, e.g. cyanates, cyanamides
- A01N47/42—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom not being member of a ring and having no bond to a carbon or hydrogen atom, e.g. derivatives of carbonic acid the carbon atom having a double or triple bond to nitrogen, e.g. cyanates, cyanamides containing —N=CX2 groups, e.g. isothiourea
- A01N47/44—Guanidine; Derivatives thereof
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23F—NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
- C23F11/00—Inhibiting corrosion of metallic material by applying inhibitors to the surface in danger of corrosion or adding them to the corrosive agent
- C23F11/08—Inhibiting corrosion of metallic material by applying inhibitors to the surface in danger of corrosion or adding them to the corrosive agent in other liquids
- C23F11/10—Inhibiting corrosion of metallic material by applying inhibitors to the surface in danger of corrosion or adding them to the corrosive agent in other liquids using organic inhibitors
- C23F11/14—Nitrogen-containing compounds
- C23F11/149—Heterocyclic compounds containing nitrogen as hetero atom
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Abstract
The invention provides a water-soluble corrosion-inhibition and sterilization integrated agent and a preparation method thereof. The corrosion inhibition and sterilization integrated agent is a brown viscous liquid intermediate product I obtained by dehydration cyclization reaction of oleic acid and diethylenetriamine in an equimolar ratio; cooling the intermediate product I to 80 ℃, adding hexamethylenediamine and guanidine hydrochloride raw materials, heating to 170-180 ℃, removing ammonia gas to perform polycondensation reaction, and adding water with the same weight as the previous material to dilute after the reaction is finished to obtain an intermediate product II; and finally, cooling the intermediate product II to below 50 ℃, and neutralizing the product to be neutral by using low carbonic acid to obtain the water-soluble corrosion-inhibition and sterilization integrated agent. The corrosion inhibition and sterilization integrated agent has the dual effects of corrosion inhibition and bacteria control, and has excellent compatibility with other agents on the oilfield site.
Description
Technical Field
The invention belongs to the field of preparation and application of corrosion inhibition bactericides, and particularly relates to a water-soluble corrosion inhibition and sterilization integrated agent and a preparation method thereof.
Background
Corrosion of metals (including Cl)-、H2S、CO2Corrosion, etc.) corrosion and bacterial slime including Sulfate Reducing Bacteria (SRB), saprophytic bacteria (TGB), iron bacteria, etc.) are one of the main causes of equipment damage in oil and gas exploitation and petrochemical industries, and the losses caused thereby are very large, and metal corrosion and bacterial slime damage have a mutually promoting relationship. There are many ways to solve the corrosion and bacteria problems, and the method using chemical agents is the simplest and most economical. Because the compatibility problem exists between different corrosion inhibitors and bactericides, and the compatibility problem also exists between the corrosion inhibitors and the bactericides and other on-site chemical agents (such as demulsifiers, scale inhibitors, flocculating agents and the like), the compatibility experiment must be carried out in advance when the corrosion inhibitors and the bactericides are applied on site, so that more troubles are caused to practical application, and the ideal treatment effect cannot be achieved frequently. Therefore, the search for an integrated chemical agent which has good corrosion inhibition performance and sterilization performance and good compatibility with other chemical agents on the oilfield site has important scientific research and economic values.
Disclosure of Invention
The invention aims to solve the problem of compatibility between different corrosion inhibitors and bactericides and the problem of compatibility between the corrosion inhibitors and the bactericides and between the bactericides and other on-site chemical agents (such as demulsifiers, flocculating agents, scale inhibitors and the like).
The technical scheme of the invention is as follows:
a preparation method of a water-soluble corrosion-inhibition and sterilization integrated agent comprises the following steps: it is characterized by having the following molecular structure:
(1) a dehydration cyclization reaction step: adding oleic acid and diethylenetriamine into a high-temperature reaction kettle with a mechanical stirrer, a condenser, a water separator, a temperature sensor and an ammonia gas absorption device in an equimolar ratio, and heating to 220-240 ℃ to enable reactants to undergo a dehydration cyclization reaction to obtain brown viscous liquid which is an intermediate product I;
(2) condensation reaction step: cooling the intermediate product I to 80 ℃, adding hexamethylenediamine and guanidine hydrochloride raw materials, wherein the molar ratio of the hexamethylenediamine to the guanidine hydrochloride to the oleic acid is 1: 10-20, heating to 170-180 ℃, removing ammonia gas to carry out polycondensation reaction for 8-10 h, and adding water with the same weight as the total amount of the materials in the early stage to dilute after the reaction is finished to obtain an intermediate product II;
(3) a neutralization reaction step: and (3) cooling the intermediate product II to below 50 ℃, and neutralizing the product to be neutral by using low carbonic acid to obtain the water-soluble corrosion-inhibition and sterilization integrated agent.
In the above preparation method, the molar ratio of hexamethylenediamine to guanidine hydrochloride is preferably 1: 1.
the preferable temperature of the dehydration ring-opening reaction is 220-230 ℃.
The invention also provides a water-soluble corrosion-inhibition and sterilization integrated agent obtained by the preparation method, which preferably has the following molecular structural formula:
wherein: n is a positive integer of 1-50;
compared with the traditional bactericide, the water-soluble corrosion-inhibition and sterilization integrated agent product has excellent corrosion inhibition (Cl)-、H2S、CO2Corrosion, etc.) and sterilization (sulfate-containing reducing bacteria (SRB), saprophytic bacteria (TGB), iron bacteria, etc.), and has excellent compatibility with other agents in the oil field.
Detailed Description
The technical solution of the present invention is further described with reference to the following specific examples.
Example 1.
Adding 282.50g (1mol) of oleic acid and 103.17g (1mol) of diethylenetriamine into a 5L high-temperature reaction kettle of a mechanical stirring device, a condenser, a water separator, a temperature sensor and an ammonia gas absorption device, heating to 220 ℃ to remove 36.00g of water, and cooling to 80 ℃ to obtain brown viscous liquid which is an intermediate I; and (3) continuously adding 1162.10g (10mol) of hexamethylene diamine and 955.30g (10mol) of guanidine hydrochloride into the reaction kettle, heating to 170 ℃, reacting for 8 hours, adding 2500g of water into the reaction kettle to dissolve the materials, then reducing the temperature of the materials to below 50 ℃, adding acetic acid to adjust the pH value of the materials to be 7-8, and obtaining the finished product.
Example 2.
Adding 282.50g (1mol) of oleic acid and 103.17g (1mol) of diethylenetriamine into a 10L high-temperature reaction kettle of a mechanical stirring device, a condenser, a water separator, a temperature sensor and an ammonia gas absorption device, heating to 240 ℃ to remove 36.00g of water, and cooling to 80 ℃ to obtain brown viscous liquid which is an intermediate I; and (3) continuously adding 2324.20g (20mol) of hexamethylene diamine and 1910.60g (20mol) of guanidine hydrochloride into the reaction kettle, heating to 175 ℃, adding 4600g of water into the reaction kettle after the reaction is carried out for 10 hours to dissolve the materials, then reducing the temperature of the materials to below 50 ℃, adding acetic acid to adjust the pH value of the materials to be 7-8, and obtaining the finished product.
Example 3.
Adding 282.50g (1mol) of oleic acid and 103.17g (1mol) of diethylenetriamine into a 10L high-temperature reaction kettle of a mechanical stirring device, a condenser, a water separator, a temperature sensor and an ammonia gas absorption device, heating to 230 ℃ to remove 36.00g of water, and cooling to 80 ℃ to obtain brown viscous liquid which is an intermediate I; and (3) continuously adding 1743.15g (15mol) of hexamethylene diamine and 1432.95g (15mol) of guanidine hydrochloride into the reaction kettle, heating to 180 ℃, adding 3500g of water into the reaction kettle after the reaction time is 9 hours to dissolve the materials, then reducing the temperature of the materials to below 50 ℃, adding acetic acid to adjust the pH value of the materials to be 7-8, and obtaining the finished product.
The obtained water-soluble corrosion-inhibition and sterilization integrated agent of examples 1-3 is evaluated for corrosion inhibition performance according to appendix B of Q/SY126-2005 technical requirements for oilfield fungicides, new sterilization performance according to technical requirements for corrosion-inhibition and scale-inhibition agents for Q/SY49-2010 oilfield water treatment, and compatibility performance according to field evaluation of certain oilfield, and the evaluation results are shown in Table 1.
TABLE 1 evaluation results of product Properties
a: evaluating according to appendix B of Q/SY126-2005 technical requirement for oilfield bactericide;
b: evaluating according to technical requirements of corrosion and scale inhibitor for Q/SY49-2010 oilfield water treatment;
c: evaluation of a certain oil field on site.
Claims (6)
1. A preparation method of a water-soluble corrosion-inhibition and sterilization integrated agent is characterized by comprising the following steps:
(1) a dehydration cyclization reaction step: adding oleic acid and diethylenetriamine into a high-temperature reaction kettle with a mechanical stirrer, a condenser, a water separator, a temperature sensor and an ammonia gas absorption device in an equimolar ratio, and heating to 220-240 ℃ to enable reactants to undergo a dehydration cyclization reaction to obtain brown viscous liquid which is an intermediate product I;
(2) condensation reaction step: cooling the intermediate product I to 80 ℃, adding hexamethylenediamine and guanidine hydrochloride raw materials, wherein the molar ratio of the hexamethylenediamine to the guanidine hydrochloride to the oleic acid is 1: 10-20, heating to 170-180 ℃, removing ammonia gas to carry out polycondensation reaction for 8-10 h, and adding water with the same weight as the total amount of the materials in the early stage to dilute after the reaction is finished to obtain an intermediate product II;
(3) a neutralization reaction step: and (3) cooling the intermediate product II to below 50 ℃, and neutralizing the product to be neutral by using low carbonic acid to obtain the water-soluble corrosion-inhibition and sterilization integrated agent.
2. The method according to claim 1, wherein the molar ratio of hexamethylenediamine to guanidine hydrochloride is 1: 1.
3. the preparation method according to claim 1, wherein the temperature of the dehydration ring-opening reaction is 220-230 ℃.
4. The method according to claim 1, wherein the lower acid in step 3) is acetic acid.
5. A water-soluble corrosion-inhibition and sterilization integrated agent prepared according to the preparation method of any one of claims 1-4.
6. The water-soluble corrosion-inhibition and sterilization integrated agent according to claim 5, characterized by having the following molecular structure:
wherein: n is a positive integer from 1 to 50.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010852267.9A CN112080002A (en) | 2020-08-21 | 2020-08-21 | Water-soluble corrosion-inhibition and sterilization integrated agent and preparation method thereof |
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| CN202010852267.9A CN112080002A (en) | 2020-08-21 | 2020-08-21 | Water-soluble corrosion-inhibition and sterilization integrated agent and preparation method thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112646558A (en) * | 2020-12-18 | 2021-04-13 | 成都劳恩普斯科技有限公司 | Ecological safety sterilization corrosion inhibitor special for shale gas pipeline and preparation method thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112646558A (en) * | 2020-12-18 | 2021-04-13 | 成都劳恩普斯科技有限公司 | Ecological safety sterilization corrosion inhibitor special for shale gas pipeline and preparation method thereof |
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Application publication date: 20201215 |